CN108120730A - A kind of hydrothermal aging evaluation method of aramid fiber - Google Patents
A kind of hydrothermal aging evaluation method of aramid fiber Download PDFInfo
- Publication number
- CN108120730A CN108120730A CN201810027800.0A CN201810027800A CN108120730A CN 108120730 A CN108120730 A CN 108120730A CN 201810027800 A CN201810027800 A CN 201810027800A CN 108120730 A CN108120730 A CN 108120730A
- Authority
- CN
- China
- Prior art keywords
- aramid fiber
- hydrothermal aging
- aging
- sample
- evaluation method
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
- G01N23/207—Diffractometry using detectors, e.g. using a probe in a central position and one or more displaceable detectors in circumferential positions
Landscapes
- Chemical & Material Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention discloses a kind of hydrothermal aging evaluation method of aramid fiber, the method step is as follows：（1）Cutting sample preparation is carried out to aramid fiber composite sample, surface is cleaned with absolute alcohol, then dries to constant weight in an oven, aramid fiber sample is divided into control group and aging group；（2）Aging group aramid fiber sample is subjected to hydrothermal aging experiment；（3）Aramid fiber sample after hydrothermal aging is tested and the aramid fiber reinforced composite sample without aging are subjected to XRD tests respectively；（4）It is that ordinate is drawn by the aramid fiber crystalline region size that abscissa, XRD tests are calculated by Scherrer formula of the hydrothermal aging time, to represent the hydrothermal aging degree of aramid fiber.The present invention is easy to operate, and sample nondestructive is hindered, and fiber crystalline region size is calculated with obtained diffraction pattern by the aramid fiber after XRD analysis hydrothermal aging, can be with the degree of aging of simple evaluation aramid fiber, and crystalline region, which tapers into, illustrates that degree of aging is gradually deepened.
Description
Technical field
The present invention relates to a kind of fibre property test method more particularly to a kind of hydrothermal aging evaluation sides of aramid fiber
Method.
Background technology
Aramid fiber is that one kind common are machine high-performance fiber, wherein being given birth to Kevlar series produced in USA and China
The F series of production is representative.Aramid fiber has better toughness and insulating properties, and has good compared to inorfil
Ripple performance, this causes aramid fiber reinforced composite to have important application in navigation and aviation field.But aramid fiber is due to structure
The problem of, can not be hardly affected by humidity as inorfil, which results in humidity be influence aramid fiber and
The important environmental factor of its composite material long-time performance.And in use, humidity often with temperature coupling,
This more accelerates the aging of aramid fiber and its composite material.At present, the research of the hydrothermal aging of aramid fiber composite material focuses mostly on
In outer layer matrix resin, discuss that the research of aramid fiber body hydrothermal aging is also rarely reported.The hydrothermal aging of aramid fiber is
A ring important in its damp-heat aging of composite material is studied, and the research of aramid fiber hydrothermal aging evaluation method is also deficient
It lacks.
Important analysis means of the X-ray diffraction as crystalline material, are widely used in each metalloid material and nonmetallic crystalline substance
In the analysis test of body material, but use it on the hydrothermal aging degree analyzing of aramid fiber, also rare research.Because aramid fiber
Fiber has apparent peak shape there are crystal region under XRD tests, and hydrothermal aging can gradually change the state of aggregation of aramid fiber
Structure, this variation can be reflected in XRD spectra, therefore can use the hydrothermal aging of XRD means of testing evaluation aramid fiber
Degree.
The content of the invention
In order to overcome the limitation of the prior art, the hydrothermal aging degree of simple accurately evaluation aramid fiber, the present invention carries
A kind of hydrothermal aging evaluation method of aramid fiber is supplied, this method is easy to operate, and sample nondestructive is hindered, passes through X-ray diffraction
（XRD）Aramid fiber after analysis hydrothermal aging calculates fiber crystalline region size with obtained diffraction pattern, can be with simple evaluation aramid fiber
The degree of aging of fiber, crystalline region, which tapers into, illustrates that degree of aging is gradually deepened.
The purpose of the present invention is what is be achieved through the following technical solutions：
A kind of hydrothermal aging evaluation method of aramid fiber, includes the following steps：
（1）Cutting sample preparation is carried out to aramid fiber composite sample, surface is cleaned with absolute alcohol, is then dried to perseverance in an oven
Weight, is divided into control group and aging group by aramid fiber sample；
（2）Aging group aramid fiber sample is put into progress hydrothermal aging experiment in deionized water；
（3）Aramid fiber sample after hydrothermal aging is tested and the aramid fiber reinforced composite sample without aging are distinguished
Carry out XRD tests；
（4）It is vertical by the aramid fiber crystalline region size that abscissa, XRD tests are calculated by Scherrer formula of the hydrothermal aging time
Coordinate plot, to represent the hydrothermal aging degree of aramid fiber.
In the present invention, the step（1）In, aramid fiber composite sample is cut into the examination for meeting size needed for XRD tests
Sample, length are 15 ~ 25 cm.
In the present invention, the step（1）In, using alcohol wipe when needs to be wiped repeatedly 3 times, and when wiping is needed fiber
Beam is broken up, and avoids the generation of capillary phenomenon as far as possible.
In the present invention, the step（1）In, when drying 24 ~ 48 is small in 50 ~ 60 DEG C of baking oven.
In the present invention, the step（1）In, it is dried to continuous three times at intervals of 4 weighing when small, fiber sample quality is exhausted
It is no more than 0.002g to error and represents that drying is completed, when this process needs 24 ~ 48 is small.
In the present invention, the step（2）In, the specific method of hydrothermal aging experiment is as follows：Aging group is vertically totally submerged
Hydrothermal aging is carried out in deionized water, the temperature of hydrothermal aging is 70 DEG C, after starting experiment, with gradual increased time interval
Sampling, ensure the degree of aging of sample has significant difference in each sample point, when total testing time is 2500 small.
In the present invention, the step（3）In, XRD test conditions are as follows：0.02 ° of test access interval, pipe presses 45 kV,
50 mA of tube current, 5 ~ 60 ° of scanning angle, 0.02 ° ~ 0.2 ° of step-length, 0.1 ° ~ 0.5 ° of second speed.
In the present invention, the step（3）In, XRD tests must as early as possible carry out after test specimen departs from ageing environment, most
Large-spacing must not exceed 12 it is small when.
In the present invention, the step（4）In, XRD test results based on obtained XRD test charts, obtain peak position with
Halfwidth is calculated using Scherrer formula, and acquired results are the mean size of crystalline region inside aramid fiber.
The invention has the advantages that：
Originally relatively fuzzy this concept of hydrothermal aging degree tool is now crystalline region size this number under XRD tests by the present invention
According to by analyzing the relation of crystalline region size variation and hydrothermal aging time, it is that a kind of aramid fiber of simple possible is wet to show this
The analysis method of heat ageing degree has the hydrothermal aging behavior of aramid fiber and its composite material under research hygrothermal environment important
Meaning.
Description of the drawings
Fig. 1 is F-12 fibers crystalline region size with ageing time variation diagram；
Fig. 2 is Kevlar-49 fibers crystalline region size with ageing time variation diagram.
Specific embodiment
Technical scheme is further described with reference to embodiment, but is not limited thereto, it is every right
Technical solution of the present invention is modified or replaced equivalently, and without departing from the spirit and scope of technical solution of the present invention, should all be contained
It covers in protection scope of the present invention.
Embodiment 1
A kind of hydrothermal aging evaluation method of aramid fiber is present embodiments provided, is as follows：
1）The preparation of aramid fiber sample
It is raw material to select F-12 fibers, is cut into the fiber sample of 25 cm of multistage, after absolute alcohol is wiped repeatedly surface 3 times,
Insert baking oven dried at 55 DEG C 36 it is small when after, be divided into control group and aging group.
2）Aging group hydrothermal aging experimental condition
The actual conditions of hydrothermal aging is 70 DEG C, and aging group sample is totally submerged in deionized water, after starting experiment, with gradual
Increased time interval sampling, ensure the degree of aging of sample has significant difference in each sample point, and total testing time is small for 2500
When.
3）XRD is tested
The sample of control sample and aging certain time is subjected to XRD tests, test condition is as follows：Test access interval
0.02 °, pipe presses 45 kV, 50 mA of tube current, 5 ~ 60 ° of scanning angle, 0.02 ° of step-length, 0.1 ° of second speed；Test ends at aging
When group disengaging ageing environment 4 is small.
4）Crystalline region size calculates
According to step 3）In the XRD that measures as a result, calculating crystalline region size, the different ageing times that will be calculated using Scherrer formula
The crystalline region size and the correspondence of time of lower F-12 fibers draw F-12 fibers crystalline region size as shown in Figure 1 with ageing time
Variation diagram.
Embodiment 2：
A kind of measuring method of water absorption rate inside aramid fiber is present embodiments provided, is as follows：
1）The preparation of aramid fiber sample
It is raw material to select Kevlar-49 fibers, is cut into the fiber sample of 20 cm of multistage, surface 3 is wiped repeatedly through absolute alcohol
After secondary, insert baking oven dried at 60 DEG C 24 it is small when after, be divided into control group and aging group.
2）Aging group hydrothermal aging experimental condition
The actual conditions of hydrothermal aging is 70 DEG C, and aging group sample is totally submerged in deionized water, after starting experiment, with gradual
Increased time interval sampling, ensure the degree of aging of sample has significant difference in each sample point, and total testing time is small for 2500
When.
3）XRD is tested
The sample of control sample and aging certain time is subjected to XRD tests, test condition is as follows：Test access interval
0.02 °, pipe presses 45 kV, 50 mA of tube current, 5 ~ 60 ° of scanning angle, 0.04 ° of step-length, 0.2 ° of second speed；Test ends at aging
When group disengaging ageing environment 3 is small.
4）Crystalline region size calculates
According to step 3）In the XRD that measures as a result, calculating crystalline region size, the different ageing times that will be calculated using Scherrer formula
The crystalline region size and the correspondence of time of lower Kevlar-49 fibers draw Kevlar-49 fibers crystalline region size as shown in Figure 2
With ageing time variation diagram.
Claims (9)
1. the hydrothermal aging evaluation method of a kind of aramid fiber, it is characterised in that the method step is as follows：
（1）Cutting sample preparation is carried out to aramid fiber composite sample, surface is cleaned with absolute alcohol, is then dried to perseverance in an oven
Weight, is divided into control group and aging group by aramid fiber sample；
（2）Aging group aramid fiber sample is put into progress hydrothermal aging experiment in deionized water；
（3）Aramid fiber sample after hydrothermal aging is tested and the aramid fiber reinforced composite sample without aging are distinguished
Carry out XRD tests；
（4）It is vertical by the aramid fiber crystalline region size that abscissa, XRD tests are calculated by Scherrer formula of the hydrothermal aging time
Coordinate plot, to represent the hydrothermal aging degree of aramid fiber.
2. the hydrothermal aging evaluation method of aramid fiber according to claim 1, it is characterised in that the step（1）In,
Aramid fiber composite sample is cut into the sample that length is 15 ~ 25 cm.
3. the hydrothermal aging evaluation method of aramid fiber according to claim 1, it is characterised in that the step（1）In,
It needs to be wiped repeatedly 3 times during using alcohol wipe, when wiping needs to break up fibre bundle.
4. the hydrothermal aging evaluation method of aramid fiber according to claim 1, it is characterised in that the step（1）In,
It is dried to continuously three times at intervals of 4 weighing when small, fiber sample quality absolute error is no more than 0.002g.
5. the hydrothermal aging evaluation method of the aramid fiber according to claim 1 or 4, it is characterised in that the step（1）
In, when drying 24 ~ 48 is small in 50 ~ 60 DEG C of baking oven.
6. the hydrothermal aging evaluation method of aramid fiber according to claim 1, it is characterised in that the step（2）In,
The specific method of hydrothermal aging experiment is as follows：Aging group, which is vertically totally submerged in deionized water, carries out hydrothermal aging, damp and hot old
The temperature of change is 70 DEG C, when total testing time is 2500 small.
7. the hydrothermal aging evaluation method of aramid fiber according to claim 1, it is characterised in that the step（3）In,
XRD test conditions are as follows：0.02 ° of test access interval, pipe presses 45 kV, 50 mA of tube current, 5 ~ 60 ° of scanning angle, step-length
0.02 ° ~ 0.2 °, 0.1 ° ~ 0.5 ° of second speed.
8. the hydrothermal aging evaluation method of aramid fiber according to claim 1, it is characterised in that the step（3）In,
XRD tests must as early as possible carry out after test specimen departs from ageing environment, when largest interval is small no more than 12.
9. the hydrothermal aging evaluation method of aramid fiber according to claim 1, it is characterised in that the step（4）In,
XRD test results obtain peak position and halfwidth based on obtained XRD test charts, are calculated using Scherrer formula, gained
As a result it is the mean size of crystalline region inside aramid fiber.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810027800.0A CN108120730A (en) | 2018-01-11 | 2018-01-11 | A kind of hydrothermal aging evaluation method of aramid fiber |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810027800.0A CN108120730A (en) | 2018-01-11 | 2018-01-11 | A kind of hydrothermal aging evaluation method of aramid fiber |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108120730A true CN108120730A (en) | 2018-06-05 |
Family
ID=62233005
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810027800.0A Pending CN108120730A (en) | 2018-01-11 | 2018-01-11 | A kind of hydrothermal aging evaluation method of aramid fiber |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108120730A (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106033055A (en) * | 2015-03-20 | 2016-10-19 | 国家电网公司 | Hydrothermal aging evaluation method of silicone rubber for composite insulator |
| CN107356518A (en) * | 2017-07-04 | 2017-11-17 | 哈尔滨工业大学 | A kind of hydrothermal aging evaluation method of aramid fiber reinforced composite |
-
2018
- 2018-01-11 CN CN201810027800.0A patent/CN108120730A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106033055A (en) * | 2015-03-20 | 2016-10-19 | 国家电网公司 | Hydrothermal aging evaluation method of silicone rubber for composite insulator |
| CN107356518A (en) * | 2017-07-04 | 2017-11-17 | 哈尔滨工业大学 | A kind of hydrothermal aging evaluation method of aramid fiber reinforced composite |
Non-Patent Citations (1)
| Title |
|---|
| 石增强: "芳纶纤维/环氧树脂的湿热老化", 《宇航材料工艺》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108508337A (en) | Dielectric analysis method for assessing XLPE cable insulation ag(e)ing state | |
| CN104515707A (en) | Temperature measurement method for electrified tensile test piece and tensile test device | |
| CN101470058A (en) | Method for evaluating residual service life of marine low-pressure rubber-insulated cable | |
| CN104330056A (en) | Method of accurately measuring cross section area of single silk and application thereof | |
| CN113884794A (en) | Method for evaluating main insulation aging state of motor wire bar | |
| CN111044391A (en) | High-temperature synchronization system and synchronization method of Hopkinson experimental equipment | |
| CN109632695A (en) | A kind of crosslinking polyethylene-insulated cable insulation ageing state characterizing method and device | |
| CN104648688A (en) | Paddle strain gauge arranging and decoupling method | |
| CN111310355B (en) | Test and analysis method for NOMEX paper life attenuation of vehicle-mounted traction transformer | |
| CN109708969A (en) | A kind of method of determining metal material anisotropy and tension and compression asymmetry feature | |
| Sekine et al. | Structural health monitoring of cracked aircraft panels repaired with bonded patches using fiber Bragg grating sensors | |
| CN105403578A (en) | Method for quickly detecting water content of bamboo on basis of X-ray CT (computed tomography) technology | |
| CN108169054B (en) | Method for measuring and calculating internal water absorption of aramid fiber | |
| CN108082534A (en) | A kind of lifting airscrew combined load test fiber arrangement and group bridge method | |
| CN108120730A (en) | A kind of hydrothermal aging evaluation method of aramid fiber | |
| CN112765776B (en) | Crosslinked polyethylene cable insulation aging state assessment method and system | |
| CN110320236A (en) | The infrared survey method of large scale wind power machine blade interior depth of defect | |
| CN203350139U (en) | High temperature rotating bending fatigue crack growth measurement device | |
| CN109507021B (en) | Method for rapidly characterizing mechanical property of composite material | |
| CN116165279B (en) | Composite insulator defect detection method, device, electronic equipment and storage medium | |
| CN105258966B (en) | A kind of lifting equipment actual time safety operating index based on crack propagation information determines method | |
| CN104913988A (en) | Hopkinson principle-based concrete axial tensile strength measuring method | |
| CN106600031A (en) | High-voltage power transmission strain clamp residual life prediction method | |
| CN115979991A (en) | Thermal barrier coating failure criterion determination method and system | |
| CN109613043A (en) | Section moisture distribution test method in a kind of chemical modification material drying process |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20180605 |
|
| RJ01 | Rejection of invention patent application after publication |